CN108097029A - A kind of preparation method of the water-fast ferric oxide desulfurizer of discrete macropore - Google Patents
A kind of preparation method of the water-fast ferric oxide desulfurizer of discrete macropore Download PDFInfo
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- CN108097029A CN108097029A CN201711476530.3A CN201711476530A CN108097029A CN 108097029 A CN108097029 A CN 108097029A CN 201711476530 A CN201711476530 A CN 201711476530A CN 108097029 A CN108097029 A CN 108097029A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/81—Solid phase processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
- B01D53/52—Hydrogen sulfide
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Abstract
The present invention relates to a kind of preparation methods of the discrete water-fast ferric oxide desulfurizer of macropore, its main preparation process is first to be mixed in a certain ratio solid solubility ferrous salt with solid hydroxide, under conditions of air is blasted, crystal seed is prepared by being co-precipitated, then the reaction was continued to glassy yellow for addition iron filings and water, a period of time is radiated in ultrasonic cleaner again, finally ferric oxide desulfurizer is obtained by filtering, washing, dry, roasting, the desulfurizing agent has the characteristics that macropore, water-fast, there is higher Sulfur capacity and intensity.
Description
Technical field
The present invention relates to a kind of water-fast de- with the water-fast ferric oxide desulfurizer of discrete macropore of high sulfur capacity and discrete macropore
The preparation method of sulphur agent belongs to processed gas field of purification.
Background technology
In coal chemical industry and petrochemical industry, due to containing a large amount of sulfide in raw material, cause in production process and discharge
Contain hydrogen sulfide in tail gas and waste water, containing hydrogen sulfide follow-up workshop section's catalyst activity component can be caused to be poisoned in production process and lost
It is living, and hydrogen sulfide directly discharge would seriously pollute the environment or even make person poultry poisoning in the tail gas and waste water discharged.
At present, researchers are researched and developed various de- always in order to reduce influence of the hydrogen sulfide to industrial production and environment
Sulfur catalyst, wherein dominant catalyst type have iron oxide type desulfurizing agent, Zinc oxide desulfurizer, and iron and manganese oxides desulfurizing agent is lived
Property charcoal desulfurizing agent and basic amine liquid desulfurizing agent etc..Wherein ferric oxide desulfurizer is the desulfurization of a kind of cheap and efficient high sulfur capacity
Agent, active component is mainly ferriferous oxide, widely used.Iron oxide desulfurization is mainly non catalytic gas solid reaction reaction, in catalyst
Surface and duct in be carried out at the same time, so caltalyst phase structure on desulfuration efficiency influence it is very big.Ferric oxide desulfurizer desulfurization
Essence is sulphur atom substitution oxygen atom, and sulphur atom is more much larger than oxygen atom, can cause if body phase aperture is too small in duct
Portion's reaction is easily blocked, and influences desulphurizing activated and Sulfur capacity, so it is mutually to improve ferric oxide desulfurizer to prepare uniform big hole body
Performance important means.This method prepares discrete macroporous iron oxide desulfurizing agent by adding in iron filings and supersonic and co-deposition.Its body
Phase duct uniformly disperses, and is spatially interspersed inside and outside Yu Tixiang, size equalization, inside also form distributed three-dimensional duct
Structure.
The content of the invention
Present invention mainly solves current ferric oxide desulfurizer aperture and pore volume are small, Sulfur capacity is not high, poor water resistance, preparation process
The problem of complexity, control condition is cumbersome, and then a kind of preparation process of invention is relatively easy, facilitate control prepares iron oxide desulfurization
The preparation method of agent, while provide a kind of iron oxide desulfurization of water-tolerant for the universal poor water resistance of ferric oxide desulfurizer
Agent.
To solve above-mentioned technical matters, the present invention provides a kind of preparation side of the discrete water-fast ferric oxide desulfurizer of macropore
Method.Its step are as follows:(a)It is 1 by iron and molar ratio hydroxy by solid solubility ferrous salt and solid hydroxide:0.7
~1:0.9 is mixed;(b)By step(a)Gained mixed material in room temperature pH=3 ~ 5 and blasts the feelings of air by coprecipitation
Crystal seed is made under condition;(c)In step(b)Iron filings are added in gained reaction product and water blasts air reaction at 75 DEG C ~ 85 DEG C
To glassy yellow;(d)By step(c)Gained reaction product is put into ultrasonic cleaner at 30 ~ 40 DEG C, and it is small that 1 ~ 2 is radiated under 28KHz
When;(e)Will steps(d)Middle gained slurry is washed and filtered;(f)By step(e)Obtained solid is dried or dried naturally;In step
(f)Middle addition auxiliary agent one and auxiliary agent two, extruded moulding, roasting again after mixing.
The present invention further discloses ferric oxide desulfurizer obtained in this way, respectively by using electron microscope into
The Morphology analysis of row microballoon and desulfurizing agent;Desulfurizing agent specific surface area analysis is carried out with n2 absorption apparatus;With X x ray diffractions
Instrument carries out desulfurizing agent material phase analysis;The porosity of desulfurizing agent is determined with mercury injection apparatus.The discrete macropore desulfurizing agent of gained
For kermesinus, crystalline phase form is α-Fe2O3, three-dimensional pore passage structure is uniform, and macropore diameter reaches 22nm, pore volume 0.53cm3/
G, specific surface area reach 66.42m2/ g, Sulfur capacity are up to 43.5%.
The invention has the advantages that:
(Ultrasonic cavitation is caused using supersonic and co-deposition during the discrete water-fast ferric oxide desulfurizer of macropore prepared by 1 present invention
Bubble and high-speed micro-jet make aperture inside iron oxide uniformly disperse and spatially be interspersed, compared with using conventional pore creating material
In the case of pore volume improve 30%;
(2)It is sub- that a certain amount of iron filings mixing sulfuric acid is added during the discrete water-fast ferric oxide desulfurizer of macropore prepared by the present invention
Molysite uses, and can dramatically increase catalyst strength and body phase aperture, intensity is up to 122N/cm, in the case of being not added with iron filings
30% is higher by, aperture also increases 40%;
(3)It first dries or dries during the discrete water-fast ferric oxide desulfurizer of macropore prepared by the present invention(90℃~110℃), then
Roasting(440℃~460℃)Two-step method, then form special discrete type body phase aperture knot due to adding in after iron filings and ultrasonic radiation
Structure causes catalyst strength and water resistance to greatly improve, using still maintaining high desulfurization activity and strong under various water vapour environments
Degree, will not dusting;
(4)In oven gas environment of the discrete water-fast ferric oxide desulfurizer of macropore prepared by the present invention available for oil phase and containing steam,
Greater activity and Sulfur capacity can be kept by being used under room temperature and medium temperature environment;
(5)The present invention adds a certain amount of K, Zn, Mg auxiliary agent, promotes Fe2 O3And K2Interaction between O, it is a small amount of right to form
The sufficiently stable more potassium ferrite KFe of water11O17 solid solutions, the promotion KFe of ZnO11O17Generation, MgFe2O4 promotes active phase point
It dissipates, so as to improve the water resistance of catalyst;
(6)The present invention adds the elements such as a certain amount of Cr, Ce, Zr, using these three elements to the interaction force of ferro element, promotees
Into the generation of distributed three-dimensional pore passage structure.
Specific embodiment:
Embodiment 1
80g ferrous sulfate and 20.8g sodium hydroxides are uniformly mixed, iron and hydroxyl molar ratio are 1:0.9, stir 40min systems
Iron oxide crystal seed is obtained, 24.2g iron filings and 240g water is added and air 50mL/min is blasted at 75 DEG C, continues to stir 60min,
Glassy yellow product is obtained, filtering is washed after placing into when 30 DEG C of radiation 1 are small in ultrasonic cleaning machine, dries, is placed into roasting case
Drying, then add the KNO of mass fraction 0.5%3, the Zn (NO of mass fraction 1.6%3)2, the Mg (NO of mass fraction 0.1%3)2, matter
Measure the Cr (NO of fraction 1.4%3)3, mass fraction 3% Ce (NO3)3, mass fraction 1.0% Zr (NO3)4, after mixing extrusion into
Type, when 350 DEG C of roastings 8 are small, you can the discrete water-fast ferric oxide desulfurizer A of macropore of the present invention is made.
Embodiment 2
80g ferrous sulfate and 19.6g sodium hydroxides are uniformly mixed, iron and hydroxyl molar ratio are 1:0.85, stir 40min systems
Iron oxide crystal seed is obtained, 24.2g iron filings and 260g water is added and air 60mL/min is blasted at 75 DEG C, continues to stir 60min,
Glassy yellow product is obtained, filtering is washed after placing into when 30 DEG C of radiation 1 are small in ultrasonic cleaning machine, dries, is placed into roasting case
Drying, then add the KNO of mass fraction 1.0%3, the Zn (NO of mass fraction 2%3)2, the Mg (NO of mass fraction 0.4%3)2, matter
Measure the Cr (NO of fraction 2%3)3, 0.5% Ce (NO3)3, mass fraction 0.8% Zr (NO3)4, extruded moulding after mixing, 600 DEG C of roastings
Burn 4 it is small when, you can be made the discrete water-fast ferric oxide desulfurizer B of macropore of the present invention.
Embodiment 3
80g frerrous chlorides and 18.4g sodium hydroxides are uniformly mixed, iron and hydroxyl molar ratio are 1:0.8, stir 35min systems
Iron oxide crystal seed is obtained, 32.2g iron filings and 280g water is added and air 80mL/min is blasted at 80 DEG C, continues to stir 60min,
Glassy yellow product is obtained, filtering is washed after placing into when 40 DEG C of radiation 1 are small in ultrasonic cleaning machine, when 90 DEG C of drying 5 are small, is placed into
Filtering is washed after roasting when 30 DEG C of radiation 1 are small in ultrasonic cleaning machine in case, is dried, places into roasting case and dries, then add matter
Measure the KNO of fraction 3.0%3, the Zn (NO of mass fraction 0.9%3)2, the Mg (NO of mass fraction 2%3)2, mass fraction 0.05%
Cr(NO3)3, mass fraction 0.1% Ce (NO3)3, mass fraction 1.2% Zr (NO3)4, extruded moulding after mixing, 500 DEG C of roastings
3 it is small when, you can be made the discrete water-fast ferric oxide desulfurizer C of macropore of the present invention.
Embodiment 4
80g frerrous chlorides and 17.3g sodium hydroxides are uniformly mixed, iron and hydroxyl molar ratio are 1:0.75, stir 40min systems
Iron oxide crystal seed is obtained, 32.2g iron filings and 300g water is added and air 80mL/min is blasted at 80 DEG C, continues to stir 60min,
Glassy yellow product is obtained, filtering is washed after placing into when 40 DEG C of radiation 1 are small in ultrasonic cleaning machine, when 100 DEG C of drying 3 are small, then is put
Enter to roast in case and dry, then add the KNO of mass fraction 1.8%3, the Zn (NO of mass fraction 1.8%3)2, mass fraction 0.1%
Mg(NO3)2, the Cr (NO of mass fraction 0.05%3)3, mass fraction 1.8% Ce (NO3)3, mass fraction 1.6% Zr (NO3)4,
Extruded moulding after mixing, when 800 DEG C of roastings 2 are small, you can the discrete water-fast ferric oxide desulfurizer D of macropore of the present invention is made.
Embodiment 5
80g ferrous sulfate and 29.0g potassium hydroxide are uniformly mixed, iron and hydroxyl molar ratio are 1:0.9, stir 40min systems
Iron oxide crystal seed is obtained, 24.2g iron filings and 240g water is added and air 50mL/min is blasted at 85 DEG C, continues to stir 60min,
Glassy yellow product is obtained, filtering is washed after placing into when 40 DEG C of radiation 2 are small in ultrasonic cleaning machine, when 90 DEG C of drying 5 are small, is placed into
It is dried in roasting case, then adds the KNO of mass fraction 5%3, the Zn (NO of mass fraction 1.2%3)2, the Mg of mass fraction 1.2%
(NO3)2, the Cr (NO of mass fraction 0.08%3)3, mass fraction 2.0% Ce (NO3)3, mass fraction 0.8% Zr (NO3)4, mix
Extruded moulding after even, when 650 DEG C of roastings 3 are small, you can the discrete water-fast ferric oxide desulfurizer E of macropore of the present invention is made.
Embodiment 6
80g ferrous sulfate and 25.8g potassium hydroxide are uniformly mixed, iron and hydroxyl molar ratio are 1:0.8, stir 50min systems
Iron oxide crystal seed is obtained, 48.3g iron filings and 300g water is added and air 50mL/min is blasted at 85 DEG C, continues to stir 60min,
Glassy yellow product is obtained, is filtered after placing into when 40 DEG C of radiation 2 are small in ultrasonic cleaning machine, when 100 DEG C of drying 3 are small, places into roasting
It is dried in saggar, then adds the KNO of mass fraction 3.5%3, the Zn (NO of mass fraction 1.8%3)2, the Mg of mass fraction 0.5%
(NO3)2, the Cr (NO of mass fraction 1.2%3)3, mass fraction 2.8% Ce (NO3)3, mass fraction 0.1% Zr (NO3)4, mix
Extruded moulding after even, when 550 DEG C of roastings 4 are small, you can the discrete water-fast ferric oxide desulfurizer F of macropore of the present invention is made.
Embodiment 7
80g frerrous chlorides and 22.6g potassium hydroxide are uniformly mixed, iron and hydroxyl molar ratio are 1:0.7, stir 45min systems
Iron oxide crystal seed is obtained, 32.2g iron filings and 280g water is added and air 50mL/min is blasted at 80 DEG C, continues to stir 60min,
Glassy yellow product is obtained, is filtered after placing into when 40 DEG C of radiation 2 are small in ultrasonic cleaning machine, when 110 DEG C of drying 2 are small, places into roasting
It is dried in saggar, then adds the KNO of mass fraction 4.2%3, the Zn (NO of mass fraction 0.5%3)2, the Mg of mass fraction 1.8%
(NO3)2, the Cr (NO of mass fraction 1.8%3)3, mass fraction 3% Ce (NO3)3, mass fraction 0.2% Zr (NO3)4, mixing
Extruded moulding afterwards, when 450 DEG C of roastings 5 are small, you can the discrete water-fast ferric oxide desulfurizer G of macropore of the present invention is made.
Embodiment 8
80g ferrous sulfate and 19.6g sodium hydroxides are uniformly mixed, iron and hydroxyl molar ratio are 1:0.85, stir 40min systems
Iron oxide crystal seed is obtained, 40.3g iron filings and 290g water is added and air 100mL/min is blasted at 80 DEG C, continue to stir
60min obtains glassy yellow product, is filtered after placing into when 40 DEG C of radiation 2 are small in ultrasonic cleaning machine, dries, place into roasting case
Middle drying, then add the KNO of mass fraction 1.0%3, the Zn (NO of mass fraction 0.1%3)2, the Mg (NO of mass fraction 1.0%3)2,
Cr (the NO of mass fraction 0.2%3)3, mass fraction 0.1% Ce (NO3)3, mass fraction 2% Zr (NO3)4, after mixing extrusion into
Type, when 350 DEG C of roastings 8 are small, you can the discrete water-fast ferric oxide desulfurizer H of macropore of the present invention is made.
In above-described embodiment 1 ~ 8, step is dried in the place of direct sunlight, and ultrasonic radiation is in 28kHz ultrasonic cleaners
Middle progress, dries and is carried out in electric drying oven with forced convection, roasts and is carried out in electric roasting furnace.
At identical conditions, to the performance of the desulfurizing agent in above-described embodiment and the conventional desulfurizing agent I obtained in the market
Tested, wherein water resistance test condition for boiling 2h see whether dusting, data are as shown in table 1.
1. desulfurizing agent performance test data of table
As it can be seen from table 1 the desulfurizing agent of the present invention has larger aperture and higher pore volume, Sulfur capacity is up to 45.2%, and resistance to
Aqueous good, the performance of each side is substantially better than desulfurizing agent product conventional in the market.
Claims (10)
1. a kind of preparation method of the water-fast ferric oxide desulfurizer of discrete macropore, includes the following steps:
(a)It is 1 by iron and molar ratio hydroxy by solid solubility ferrous salt and solid hydroxide:0.7~1:0.9 carries out
Mixing;
(b)By step(a)Crystalline substance is made by coprecipitation in room temperature pH=3 ~ 5 and in the case of blasting air in gained mixed material
Kind;
(c)In step(b)Iron filings are added in gained reaction product and water blasts air reaction to glassy yellow at 75 DEG C ~ 85 DEG C;
(d)Will steps(c)Products therefrom be put into ultrasonic cleaning machine 40 DEG C of radiation 1 ~ 2 it is small when;
(e)By step(d)Gained slurry is washed and filtered;
(f)By step(e)Obtained solid is dried or dried naturally;
(g)In step(f)Middle addition auxiliary agent one and auxiliary agent two, extruded moulding, roasting again after mixing.
2. according to the method described in claim 1, it is characterized in that:Step(a)The solid solubility ferrous salt is sub- for sulfuric acid
One or more of iron, ferrous nitrate, ferrous phosphate or frerrous chloride, the solid hydroxide are sodium hydroxide or hydrogen-oxygen
Change potassium.
3. according to the method described in claim 1, it is characterized in that:Step(a)The solid solubility ferrous salt is preferably sulphur
Sour ferrous or frerrous chloride.
4. preparation method according to claim 1, it is characterised in that:Step(b)In coprecipitation be to be stirred by machinery
Completion is mixed, mixing time is 40 ~ 60 minutes, and the amount for blasting air is 50 ~ 100mL/min.
5. preparation method according to claim 1, it is characterised in that:Step(c)In iron filings mole be step(a)In
1.5 ~ 3 times of ferrous mole, step(c)In water quality be step(a)3 ~ 4 times of middle ferrous iron mole.
6. preparation method according to claim 1, it is characterised in that:Step(d)Middle ultrasonic cleaner temperature is set as
30 DEG C ~ 40 DEG C, radiation frequency 28kHz, power 200w, when the time is 1 ~ 2 small.
7. preparation method according to claim 1, it is characterised in that:Step(f)Dry temperature naturally as 25 DEG C ~ 65
DEG C, drying temperature is 90 DEG C ~ 110 DEG C.
8. preparation method according to claim 1, it is characterised in that:Step(g)In auxiliary agent one be KNO3、Zn(NO3)2、
Mg(NO3)2, KNO3Additive amount be mass fraction 0.5 ~ 5%, Zn (NO3)2Additive amount be mass fraction 0.1 ~ 2%, Mg (NO3)2Addition
It measures as mass fraction 0.1 ~ 2%.
9. preparation method according to claim 1, it is characterised in that:Step(g)In auxiliary agent two be Cr (NO3)3、Ce
(NO3)3、Zr(NO3)4, Cr (NO3)3Additive amount is mass fraction 0.05 ~ 2%, Ce (NO3)3Additive amount for mass fraction 0.1 ~ 3%,
Zr(NO3)4Additive amount is mass fraction 0.1 ~ 2%.
10. preparation method according to claim 1, it is characterised in that:Step(g)In calcination temperature for 350 ~ 800 DEG C,
Time is 2 ~ 8h.
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Address after: 430223, building 6, building 18, Chinese workers' science and Technology Park, East Lake Development Zone, Wuhan, Hubei Applicant after: Wuhan Kelin Chemical Industry Group Co.,Ltd. Address before: 430223, building 6, building 18, Chinese workers' science and Technology Park, East Lake Development Zone, Wuhan, Hubei Applicant before: WUHAN KELIN FINE CHEMICAL Co.,Ltd. |
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GR01 | Patent grant | ||
GR01 | Patent grant |